CN101176726A - Medicine-loading sustained-release micro-capsule and preparing method thereof - Google Patents
Medicine-loading sustained-release micro-capsule and preparing method thereof Download PDFInfo
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Abstract
The utility model relates to a new drug-loading controlled-releasing microcapsule and a preparation method thereof, which belongs to the field of the material preparation and the medicine application, and is expected to have applications in the filed of the food, the spice, the makeup, the pesticide, the organism and other fields. A new micro encapsulant system of medicine / silicon dioxide with the core-shell composite structure is prepared by means of the emulsion in-situ encapsulation and synthesis, and can embed the medicine with different molecular dimensions into the cavity, that makes the new micro encapsulant system become a warehouse for medicine storage indeed, and increases the medicine load; and the release rate of the medicine can be regulated by means of the shell structure to reach the goal of slow release.
Description
Technical field:
The present invention relates to a kind of carried medicine sustained-release microcapsule and preparation method thereof.Relate to material preparation and medical applications field, and be expected to be applied to fields such as food, spice, cosmetics, pesticide, biology.
Background technology:
In recent years, the medicament slow release technology since have can prolong drug release time, improve drug effect, reduce medication number of times and drug side effect, prevent advantage such as drug degradation, attracted to pay close attention to widely.
At present, most widely used aspect the preparation of slow releasing pharmaceutical be microcapsule technology, promptly adopt the capsule materials/substances that medicine and capsule-core material are coated the formation microcapsule, must see through cyst wall during drug release, thereby reach the effect of slow release.Yet, the complicated process of preparation of traditional microcapsule, raw material type is many, and slow release effect is influenced by formula for a product not only, is also prepared process influence, and general slow release process only continues a few hours to tens hour, can't satisfy the slow release requirement of longer time.
Another preparation method that extensively adopts is the load method, is about to the pharmaceutically active molecule and loads on the carrier mass by physics or chemical action, and the product slow release effect that this method obtains is better.Which kind of method no matter, present widely used capsule materials/substances or carrier mass mainly are various natural or synthetic high molecular polymers.Because the problem that aspects such as polymer self property limitation and biocompatibility thereof exist, its application also just is restricted.
Earth silicon material also is applied to this field, for we provide another kind of selection in recent years gradually owing to have good stable and biocompatibility.At present, people can synthesize the silicon dioxide of multiple pattern, and are applied to the medicament slow release field.Document [1] (Vallet-Regi M, Ramila A, del Real R P, Perez-Pariente J.A New Property of MCM-41:Drug DeliverySystem[J] .Chem Mater, 2001,13:308-311) proposed the novel mesopore molecular sieve that a kind of application has nanostructured and prepared slow releasing pharmaceutical as carrier, the interaction between its Chinese medicine and the carrier is based on physical absorption; Document [2] (Song SW, Hidajat K, Kawi S.Functionalized SBA-15Materials as Carriers for Controlled Drug Delivery:Influence of SurfaceProperties on Matrix-Drug Interactions[J] .Langmuir, 2005,21 (21): 9568-9575) proposed a kind of SBA-15 of utilization type mesoporous silicon oxide as pharmaceutical carrier, introduce active group by surface modification, make the stronger hydrogen bond of generation between medicine and carrier etc. be used for improving sustained release performance; Document [3] (Chen JF, Ding HM, Wang JX, Shao L.Preparation and characterization ofporous hollow silica nanoparticles for drug delivery application[J] .Biomaterials, 2004,25 (4): 723-727) proposed a kind of hollow-core construction silicon dioxide of novelty as pharmaceutical carrier, its special hollow-core construction can be used as the warehouse of medicine storage, therefore can significantly increase drug loading, and have the advantage of microcapsule-type and support type slow releasing agent concurrently, reach the good slow release effect.Yet adopting silicon dioxide at present mainly is to prepare carrier silicon dioxide earlier as the preparation of drug carriers method, again by other means such as dippings, supercritical with the two-step method of drug loading to the carrier.The shortcoming of this method is that the payload of medicine is subjected to the influence of drug molecule size, carrier surface pore passage structure and size very big.The medicine bigger to molecular dimension, the embedding amount that commonsense method obtained is lower, and drug molecule almost can't enter the duct, more can't be stored in hollow-core construction inside by passing hole channel, so slow release effect is had a greatly reduced quality also.From document [4] (Zhu YF, Shi JL, Li YS, Chen HR, Shen WH, Dong XP.Hollowmesoporous spheres with cubic pore network as a potential carrier for drugstorage and its in vitro release kinetics[J] .J.Mater.Res., 2005,20 (1): result 54-61) as can be known, the load capacity of medicine gentamycin sulfate on hollow meso-porous titanium dioxide silicon carrier only has 12%, and most of medicine is adsorbed on carrier surface, promptly discharges fully in 3 hours.Slow-release period is short, makes the effective acting time of medicine short, can not satisfy the demand.
Summary of the invention:
One of purpose of the present invention provides a kind of novel carried medicine sustained-release microcapsule with bigger drug loading, good slow release performance and biocompatibility.
Two of purpose of the present invention provides a kind of preparation method of new sustained release microcapsule, prepare medicine/silicon dioxide novel microcapsules system by the emulsion by in-situ coating with synthetic method with nucleocapsid composite construction, the pharmaceutical pack of different molecular size can be embedded in hollow interior, make it really become the warehouse of medicine storage, improve the drug loading amount, and can utilize shell structurre to regulate drug release rate, reach the purpose of slow release.
The invention main points:
The novel carried medicine sustained-release microcapsule of the present invention, for having the microsphere of nucleocapsid composite construction, its shell material is the silicon dioxide with loose structure, and kernel is an active constituents of medicine, and drug loading is 10～30% in mass.
The preparation method of the novel carried medicine sustained-release microcapsule of the present invention for emulsion by in-situ coats and synthetic method, specifically may further comprise the steps:
A is dissolved in medicine in the aqueous solution that contains precipitant, and adds the water soluble surfactant active, and mix homogeneously forms the water solution A of medicine-surfactant-precipitant;
B adds oil soluble surfactant in the water-fast non-polar oil solvent, and mix homogeneously forms the solution B of surfactant-oil solvent;
C slowly adds solution A in the solution B under stirring condition, continues stirring until to form stable water/oil type emulsion C; Wherein the volume ratio of solution A and solution B is 1: 100～1: 2, is preferably 1: 50～1: 10;
D adds siloxanes eka-silicon source material in emulsion C, and continues to stir, and mixing time is 2～72 hours, is preferably 10～48 hours, makes abundant hydrolysis of silicon source material and polycondensation, forms the coated with silica layer on oil-water interfaces;
E filters, the core-shell particles slow-release microcapsule of medicine that obtained embedding after washing and the drying.Washing process can according to circumstances carry out repeatedly, can adopt dehydrated alcohol or washing with acetone, its objective is the removal residual surfactant
Said medicine is water-soluble medicine, replenishes class (as potassium chloride) or asthma class medicine (as aminophylline, salbutamol sulfate) comprising antibiotics (as gentamycin sulfate), analgesia class (example hydrochloric acid tramadol, morphine sulfate, diclofenac sodium), blood pressure lowering class (as spectinomycin hydrochloride), anti-anemia class (as ferrous sulfate), electrolyte.
Said precipitant is sulphuric acid, hydrochloric acid or nitric acid, and the mass fraction of precipitant in solution A is 1%～10%, preferred 3%～6%.
The used water soluble surfactant active of step a is a kind of in Polyoxyethylene Sorbitol Fatty Acid Esters class or the polyoxyethylene sorbitan fatty acid ester surfactant or their mixture, and the concentration in solution A is 0～0.1g/ml; The used oil soluble surfactant of step b is a kind of in Span class or the sorbitan fatty acid ester class surfactant or their mixture, and the concentration in solution B is 0～0.3g/ml.
Said non-polar oil solvent is normal hexane, normal heptane, cyclohexane extraction, ether, dichloromethane or chloroform among the step b.
Said siloxanes eka-silicon source material is methyl silicate or ethyl orthosilicate in the steps d, and its consumption is counted 5～40% of water with the silicon dioxide quality, is preferably 20～30%.
The concentration of solution A Chinese medicine is 20～1000mg/ml, is preferably 80～200mg/ml.In addition, the microcapsule drug loading can be controlled by the concentration of regulator solution A Chinese medicine.
The whole process of preparation principle is: silicon source material (methyl silicate or ethyl orthosilicate) is met water, and hydrolysis can take place, and its intramolecular four alkoxyls can progressively become hydroxyl, acts on by polycondensation, crosslinked etc. afterwards and forms amorphous silica.This method adds silicon source material in the oil phase of entry/fat liquor, make it slowly be diffused on the oil-water interfaces and meet the water hydrolysis, when its partial hydrolysis, owing to have lipophilic alkoxyl and hydrophilic hydroxyl simultaneously, therefore can rest on the oil-water interfaces and polycondensation takes place, thereby form the silicon dioxide spherical shell on the emulsion droplet surface, pharmaceutical pack is overlayed on inside.
The effect of surfactant mainly is to make emulsion-stabilizing in the preparation process, coalescence can not take place in preparation process, divide to equate change and influence the coating process and carry out.Surfactant can only add in water or oil phase, all adds in also can be biphase.When adding two kinds of surfactants, its objective is composite good emulsifying and the stablizing effect of reaching by two kinds of surfactants.
The main effect of precipitant is the hydrolysis of quickening silicon source material.When precipitant existed, the hydrolysis rate of silicon source material can obviously be accelerated, and the response time also shortens significantly.Simultaneously, can control the hydrolysis rate of silicon source material by the addition of control precipitant.
The invention effect:
Adopt the infrared spectrum analysis of the novel carried medicine sustained-release microcapsule product of method gained of the present invention to show between medicine and the coated with silica layer not have chemical action.The pore-size distribution measurement result shows, drug-loading microcapsule is similar to the blank hollow silica ball pore-size distribution after the calcining, pore volume is more or less the same, therefore can know drug main by inference will be distributed in hollow-core construction inside, be the nucleocapsid composite construction, hollow-core construction is the real repository of medicine, can not only improve medicine embedding amount, slow-release period that can also prolong drug.Experimental results show that by external stripping: slow-release microcapsule of the present invention has the good slow release performance, and drug release is type first quick and back slow.Medication initial stage drug release is very fast, helps reaching rapidly onset concentration; Drug release is mild afterwards, helps keeping for a long time onset concentration.Because porous silica has good physicochemical performance and biocompatibility, therefore this microcapsule can not only reach the good slow release effect, also can avoid the toxic action of high-molecular organic material to human body.
Description of drawings:
Fig. 1 is the electron scanning micrograph of the embodiment of the invention 1 gained new sustained release microcapsule
As seen from Figure 1, the prepared new sustained release microcapsule spheroidal particle that is particle diameter 3～15 μ m.
Fig. 2 is the thermogravimetric analysis figure of the embodiment of the invention 1 gained new sustained release microcapsule
Fig. 3 is the infrared spectrogram of the embodiment of the invention 1 gained new sustained release microcapsule
Spectrogram 3 is blank silicon dioxide infrared spectrum among the figure, and spectrogram 4 is a gentamycin sulfate crude drug infrared spectrum, and spectrogram 5 is the infrared spectrum of new sustained release microcapsule.The three contrasts as can be known, and chemical action does not take place for medicine and silicon dioxide.
Fig. 4 is the external stripping curve of the embodiment of the invention 1 gained new sustained release microcapsule
As seen from the figure, the slowly-releasing process of this slow-release microcapsule is type first quick and back slow, and medication initial stage medicine discharges Comparatively fast, be conducive to reach rapidly onset concentration; Medicine discharges gently afterwards, is conducive to keep for a long time Effect concentration. Release amount of medicine can reach that release amount of medicine can in 48%, 4 hour of total embedding amount in 1 hour Reaching release amount of medicine in 55%, 12 hour of total embedding amount can reach in 63%, 36 hour of total embedding amount Release amount of medicine can reach that release amount of medicine can reach 70 of total embedding amount in 67%, 60 hour of total embedding amount More than the %.
The specific embodiment:
Embodiment 1: it is 6% hydrochloric acid that 0.2g medicine gentamycin sulfate is dissolved in the 2ml mass fraction, and adding 0.04g water soluble surfactant active polyoxyethylene 20 sorbitan monooleate, mix homogeneously forms the water solution A of medicine-surfactant-precipitant, wherein drug level is about 100mg/ml, and water soluble surfactant active's concentration is about 0.02g/ml; 2.0g oil soluble surfactant sorbitan monooleate is added in the water-fast non-polar oil solvent of the 50ml cyclohexane extraction, and mix homogeneously forms the solution B of surfactant-oil solvent, and wherein the concentration of oil soluble surfactant is about 0.04g/ml; Under stirring condition, solution A is slowly added in the solution B, the volume ratio of solution A and solution B is 1: 25, continues stirring until to form stable water/oil type emulsion C; In emulsion C, add silicon source material ethyl orthosilicate 2ml (by the water solution A quality 25%), and continue to stir 24 hours, make abundant hydrolysis of silicon source material and polycondensation, on oil-water interfaces, form the coated with silica layer; Solid collected by filtration after 50 ℃ of following dryings, is dispersed in the dehydrated alcohol again, and filtration drying obtains having the slow-release microcapsule of nucleocapsid composite construction once more.The medication amount that is coated is about 17% (medication amount that is coated is meant that the quality of medicine accounts for the ratio of slow-release microcapsule quality).
Embodiment 2: to the 2ml mass fraction is to add 0.4g medicine gentamycin sulfate and 0.04g water soluble surfactant active polyoxyethylene 20 sorbitan monooleate in 6% the hydrochloric acid, mix homogeneously forms the water solution A of medicine-surfactant-precipitant, wherein drug level is about 200mg/ml, and water soluble surfactant active's concentration is about 0.02g/ml; Other gets 2.0g oil soluble surfactant sorbitan monooleate, is dissolved in the water-fast non-polar oil solvent of the 50ml cyclohexane extraction, and mix homogeneously forms the solution B of surfactant-oil solvent, and wherein the concentration of oil soluble surfactant is about 0.04g/ml; Under stirring condition, solution A is slowly added in the solution B, the volume ratio of solution A and solution B is 1: 25, continues stirring until to form stable water/oil type emulsion C; In emulsion C, add silicon source material ethyl orthosilicate 2ml (by the water solution A quality 25%), and continue to stir 30 hours, make abundant hydrolysis of silicon source material and polycondensation, on oil-water interfaces, form the coated with silica layer; Solid collected by filtration after 50 ℃ of following dryings, is dispersed in the dehydrated alcohol again, and filtration drying obtains having the slow-release microcapsule of nucleocapsid composite construction once more.The medication amount that is coated is about 29%.
Embodiment 3: it is in 6% the hydrochloric acid that 0.2g medicine salbutamol sulfate is dissolved in the 2ml mass fraction, and adding 0.04g water soluble surfactant active polyoxyethylene 20 sorbitan monooleate, mix homogeneously forms the water solution A of medicine-surfactant-precipitant, wherein drug level is about 100mg/ml, and water soluble surfactant active's concentration is about 0.02g/ml; 2.0g oil soluble surfactant sorbitan monooleate is added in the water-fast non-polar oil solvent of the 50ml cyclohexane extraction, and mix homogeneously forms the solution B of surfactant-oil solvent, and wherein the concentration of oil soluble surfactant is about 0.04g/ml; Under stirring condition, solution A is slowly added in the solution B, the volume ratio of solution A and solution B is 1: 25, continues stirring until to form stable water/oil type emulsion C; In emulsion C, add silicon source material ethyl orthosilicate 2ml (by the water solution A quality 25%), and continue to stir 24 hours, make abundant hydrolysis of silicon source material and polycondensation, on oil-water interfaces, form the coated with silica layer; Solid collected by filtration after 50 ℃ of following dryings, is dispersed in the dehydrated alcohol again, and filtration drying obtains having the slow-release microcapsule of nucleocapsid composite construction once more.The medication amount that is coated is about 13%.
Embodiment 4: to the 2ml mass fraction is to add 0.2g medicine gentamycin sulfate and 0.06g water soluble surfactant active polyoxyethylene 20 sorbitan monooleate in 6% the nitric acid, mix homogeneously forms the water solution A of medicine-surfactant-precipitant, wherein drug level is about 100mg/ml, and water soluble surfactant active's concentration is about 0.03g/ml; Other gets 2.5g oil soluble surfactant sorbitan monooleate, is dissolved in the water-fast non-polar oil solvent of the 50ml normal heptane, and mix homogeneously forms the solution B of surfactant-oil solvent, and wherein the concentration of oil soluble surfactant is about 0.05g/ml; Under stirring condition, solution A is slowly added in the solution B, the volume ratio of solution A and solution B is 1: 25, continues stirring until to form stable water/oil type emulsion C; In emulsion C, add silicon source material ethyl orthosilicate 2ml (by the water solution A quality 25%), and continue to stir 48 hours, make abundant hydrolysis of silicon source material and polycondensation, on oil-water interfaces, form the coated with silica layer; Solid collected by filtration after 50 ℃ of following dryings, is dispersed in the dehydrated alcohol again, and filtration drying obtains having the slow-release microcapsule of nucleocapsid composite construction once more.The medication amount that is coated is about 15%.
Embodiment 5: it is in 6% the hydrochloric acid that 0.5g medicine gentamycin sulfate and 0.10g water soluble surfactant active polyoxyethylene 20 sorbitan monooleate are dissolved in the 5ml mass fraction, mix homogeneously forms the water solution A of medicine-surfactant-precipitant, wherein drug level is about 100mg/ml, and water soluble surfactant active's concentration is about 0.02g/ml; 5.0g oil soluble surfactant sorbitan monooleate is added in the water-fast non-polar oil solvent of the 50ml normal hexane, and mix homogeneously forms the solution B of surfactant-oil solvent, and wherein the concentration of oil soluble surfactant is about 0.1g/ml; Under stirring condition, solution A is slowly added in the solution B, the volume ratio of solution A and solution B is 1: 10, continues stirring until to form stable water/oil type emulsion C; In emulsion C, add silicon source material ethyl orthosilicate 5ml (by the water solution A quality 25%), and continue to stir 20 hours, make abundant hydrolysis of silicon source material and polycondensation, on oil-water interfaces, form the coated with silica layer; Solid collected by filtration after 50 ℃ of following dryings, is dispersed in the dehydrated alcohol again, and filtration drying obtains having the slow-release microcapsule of nucleocapsid composite construction once more.The medication amount that is coated is about 15%.
Embodiment 6: to the 2ml mass fraction is to add 0.2g medicine gentamycin sulfate and 0.04g water soluble surfactant active polyoxyethylene 20 sorbitan monopalmitate in 6% the hydrochloric acid, mix homogeneously forms the water solution A of medicine-surfactant-precipitant, wherein drug level is about 125mg/ml, and water soluble surfactant active's concentration is about 0.02g/ml; Other gets 2.0g oil soluble surfactant sorbitan monooleate, is dissolved in the water-fast non-polar oil solvent of the 50ml cyclohexane extraction, and mix homogeneously forms the solution B of surfactant-oil solvent, and wherein the concentration of oil soluble surfactant is about 0.04g/ml; Under stirring condition, solution A is slowly added in the solution B, the volume ratio of solution A and solution B is 1: 25, continues stirring until to form stable water/oil type emulsion C; In emulsion C, add silicon source material ethyl orthosilicate 2.4ml (by the water solution A quality 30%), and continue to stir 30 hours, make abundant hydrolysis of silicon source material and polycondensation, on oil-water interfaces, form the coated with silica layer; Solid collected by filtration after the drying, is dispersed in the dehydrated alcohol under 50C again, and filtration drying obtains having the slow-release microcapsule of nucleocapsid composite construction once more.The medication amount that is coated is about 12%.
Embodiment 7: it is in 6% the hydrochloric acid that 0.5g medicine gentamycin sulfate and 0.40g water soluble surfactant active polyoxyethylene 20 sorbitan monopalmitate are dissolved in the 5ml mass fraction, mix homogeneously forms the water solution A of medicine-surfactant-precipitant, wherein drug level is about 100mg/ml, and water soluble surfactant active's concentration is about 0.08g/ml; 1.6g oil soluble surfactant sorbitan trioleate is added in the water-fast non-polar oil solvent of the 50ml cyclohexane extraction, and mix homogeneously forms the solution B of surfactant-oil solvent, and wherein the concentration of oil soluble surfactant is about 0.03g/ml; Under stirring condition, solution A is slowly added in the solution B, the volume ratio of solution A and solution B is 1: 10, continues stirring until to form stable water/oil type emulsion C; In emulsion C, add silicon source material ethyl orthosilicate 5ml (by the water solution A quality 25%), and continue to stir 48 hours, make abundant hydrolysis of silicon source material and polycondensation, on oil-water interfaces, form the coated with silica layer; Solid collected by filtration after 50 ℃ of following dryings, is dispersed in the dehydrated alcohol again, and filtration drying obtains having the slow-release microcapsule of nucleocapsid composite construction once more.The medication amount that is coated is about 15%.
Embodiment 8: to the 2ml mass fraction is to add 0.2g medicine gentamycin sulfate in 6% the hydrochloric acid, and dissolving and mix homogeneously form the water solution A of medicine-precipitant, and wherein drug level is about 100mg/ml; Other gets 8.0g oil soluble surfactant sorbitan monooleate, is dissolved in the water-fast non-polar oil solvent of the 30ml cyclohexane extraction, and mix homogeneously forms the solution B of surfactant-oil solvent, and wherein the concentration of oil soluble surfactant is about 0.27g/ml; Under stirring condition, solution A is slowly added in the solution B, the volume ratio of solution A and solution B is 1: 15, continues stirring until to form stable water/oil type emulsion C; In emulsion C, add silicon source material ethyl orthosilicate 2ml (by the water solution A quality 25%), and continue to stir 12 hours, make abundant hydrolysis of silicon source material and polycondensation, on oil-water interfaces, form the coated with silica layer; Solid collected by filtration after 50 ℃ of following dryings, is dispersed in the dehydrated alcohol again, and filtration drying obtains having the slow-release microcapsule of nucleocapsid composite construction once more.The medication amount that is coated is about 15%.
Embodiment 9: it is in 3% the hydrochloric acid that 0.2g medicine gentamycin sulfate is dissolved in the 2ml mass fraction, and adding 0.04g water soluble surfactant active polyoxyethylene 20 sorbitan monooleate, mix homogeneously forms the water solution A of medicine-surfactant-precipitant, wherein drug level is about 100mg/ml, and water soluble surfactant active's concentration is about 0.02g/ml; 2.0g oil soluble surfactant sorbitan monooleate is added in the water-fast non-polar oil solvent of the 50ml cyclohexane extraction, and mix homogeneously forms the solution B of surfactant-oil solvent, and wherein the concentration of oil soluble surfactant is about 0.04g/ml; Under stirring condition, solution A is slowly added in the solution B, the volume ratio of solution A and solution B is 1: 25, continues stirring until to form stable water/oil type emulsion C; In emulsion C, add silicon source material ethyl orthosilicate 1.6ml (by the water solution A quality 20%), and continue to stir 48 hours, make abundant hydrolysis of silicon source material and polycondensation, on oil-water interfaces, form the coated with silica layer; Solid collected by filtration after drying under 50 ℃ of C, is dispersed in the dehydrated alcohol again, and filtration drying obtains having the slow-release microcapsule of nucleocapsid composite construction once more.The medication amount that is coated is about 17%.
Claims (10)
1. novel carried medicine sustained-release microcapsule, for having the microsphere of nucleocapsid composite construction, its shell material is the silicon dioxide with loose structure, and kernel is an active constituents of medicine, and drug loading is 10～30% in mass.
2. the preparation method of the described carried medicine sustained-release microcapsule of claim 1 is emulsion by in-situ coating and synthetic method, specifically may further comprise the steps:
A is dissolved in medicine in the aqueous solution that contains precipitant, and adds the water soluble surfactant active, and mix homogeneously forms the water solution A of medicine-surfactant-precipitant;
B adds oil soluble surfactant in the water-fast non-polar oil solvent, and mix homogeneously forms the solution B of surfactant-oil solvent;
C slowly adds solution A in the solution B under stirring condition, and the volume ratio of solution A and solution B is 1: 100～1: 2, continues stirring until to form stable water/oil type emulsion C;
D adds siloxanes eka-silicon source material in emulsion C, and continues to stir, and makes abundant hydrolysis of silicon source material and polycondensation, forms the coated with silica layer on oil-water interfaces;
E filters, the core-shell particles slow-release microcapsule of medicine that obtained embedding after washing and the drying.
3. according to the preparation method of claim 2, it is characterized in that: said medicine is water-soluble antibiotics, analgesia class, blood pressure lowering class, anti-anemia class, the additional class of electrolyte or asthma class medicine, and the concentration of solution A Chinese medicine is 20～1000mg/ml; Said non-polar oil solvent is normal hexane, normal heptane, cyclohexane extraction, ether, dichloromethane or chloroform among the step b.
4. according to the preparation method of claim 3, it is characterized in that: the concentration of solution A Chinese medicine is 80～200mg/ml.
5. according to the preparation method of claim 2, it is characterized in that: the volume ratio of solution A and solution B is 1: 50～1: 10 among the step c.
6. according to the preparation method of claim 2, it is characterized in that: said precipitant is sulphuric acid, hydrochloric acid or nitric acid, and the mass fraction of precipitant in solution A is 1%～10%.
7. according to the preparation method of claim 6, it is characterized in that: the mass fraction of precipitant in solution A is 3%～6%.
8. according to the preparation method of claim 2, it is characterized in that: the used water soluble surfactant active of step a is a kind of in Polyoxyethylene Sorbitol Fatty Acid Esters class or the polyoxyethylene sorbitan fatty acid ester surfactant or their mixture, and the concentration in solution A is 0～0.1g/ml; The used oil soluble surfactant of step b is a kind of in Span or the sorbitan fatty acid ester class surfactant or their mixture, and the concentration in solution B is 0～0.3g/ml.
9. according to the preparation method of claim 2, it is characterized in that: said siloxanes eka-silicon source material is methyl silicate or ethyl orthosilicate in the steps d, and its consumption is counted 5～40% of water with the silicon dioxide quality, and mixing time is 2～72 hours.
10. according to the preparation method of claim 9, it is characterized in that: said siloxanes eka-silicon source material consumption is counted 20～30% of water by the silicon dioxide quality in the steps d, and mixing time is 10～48 hours.
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